N-bromobutanimide → 1,5-Dibromo-2,4-difluorobenzene

A total of 1.6 g of 1-bromo-2,4-difluorobenzene was suspended in 8.29 ml of sulfuric acid, and 1.62 g of N-bromosuccinimide was added under ice-cooling. After stirring at room temperature for 17 hours, the reaction mixture was poured onto ice-water and extracted with ethyl acetate. The resulting organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and brine, dried over magnesium sulfate and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (hexane), to give 2.18 g of the title compound as a pale yellow oil.

1. temperaturecooling
2. additionthe reaction mixture was poured onto ice-water
3. extractionextracted with ethyl acetate
4. washThe resulting organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and brine
5. dry with materialdried over magnesium sulfate
6. customthe solvent was evaporated
7. customThe residue was purified
8. customseparated by silica gel column chromatography (hexane)

ORD record

ord-33d6220b1fb24ca592b03ce7a8920c2b

Source dataset

uspto-grants-2006_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06982274B2